Distilling head



May-:19419v Gl-'DSBARRY ETAL/ .DIS'TILLING HEAD filed Jan, 1, y1945 v y? Y? .Ef MM W ,n e w Patented May 3, 1949 DISTILLING vAlbert W; Goldsbarryg Northbrook,andHowardvS. Martin, Glenview, Ill., assignors to The Pure Oil Company, Chicago, Ill., a corporation of "Ohio Application January 1, 1945, Seria'l'No. 5705918 This invention relates `to improvement in :a glass distilling yhead .for use -in connection with laboratory distillation apparatus.

In vPatent No. 2,251,185 there is disclosed a reflux control appar-atus tor Ause on a fractional dstilling column. wThe distilling head disclosed inthe aforesaid` patent yhas several disadvantages. The principal ydisadvantage is that the vapors from the distilling-col-umn enter the section surrounding the swinging funnel and Vare partially condensed and returned to the fractionatlng column without vpassing .through the funnel so that it is not possible to accurately regulate the amountof reflux liquid which is returned to the -distilling column. Another disadvantage is that the funnelis supportedvonlglass .lugs -formed lon the inside ofthe fractionatinghead which tend to wear and interfere with the free swinging of the funnel. If the product being subjected to distillation contains gum formers, gum has a tenfdency to deposit on the supporting lugs and around the studs whichsupport the funnel, thereby further interfering with the free opera-tion of the funnel. Aiurther objection to the distilling head shown in the vaforesaid patent, is that it lis made .in one piece with the result that breakv.age of a portion thereof requires replacement of the whole head. Still another objection to the distilling head shown fand-described in the aforesaid patent is that it Aispprovfided with `a stopcock :in the pressure equalizer line Il which must ,be turned in order to draw oli `reux from the distilling head. If the stopcock is inadvertently Atur-ned in the wrong direction, the pressure :bal- .ance between the top and the bottom of the .head is destroyed.

The object of our invention is to provide a distilling head which obviates the aforesaid disadvantages as well as other :disadvantages which will become apparent yfrom the following description and accompanying-drawing of which Figure 1 is a diagrammatic, Aelevational view .of adistilling head constructed in accordance with our invention, and

`Figure 2 is a fragmentary detail of the swinging funnel forming part of the apparatus, in diagrammatic, elevation looking at the apparatus 4from Aan angle 90 fromzthe direction in which Figure I1 is Viewed.

,Referring tothe drawing, numeral 4 indicates an annular evacuated jacketconstructed varound an axial vapor passage 3,-the upper end 5 of which is restricted and vslightly taperedoutwardly from lbottorn to top. The surface of the tapered portion-5 isground in order to `snugly accomlll mod-ate .and formv a leak-proof loint'with vather- .mocouple ortherniometerwell l extendingdownwardly into the passageway f3 to ta point below the point of Vapor-exit therefrom. `Athermocouple -or thermometer (not shown) is adapted to .be inserted into the thermocou-ple well in order to .measure the temperature of the vapors at the point where they :lea-ye the passageway 3.

The bottom 9 yof the jacket l is circular jin cross-section and-gradually tapers yinwardly .from the point ll to the point i3. The :surface of the portion El is ground in order that itmayterm fa vapor-tight joint when inserted into the top of a conventional glass .fractional distillation -column.

A horizontally vdisposed tube lI5 connects the upper end of the passageway 3 `'at .a point immediately below the restricted lupper end -5 with a condenser l1. The tube l5 `is fused to the wall of both the passageway and the jacketA I.. The condenser I1 is enclosed `in a `water jacket |39 provided with water` inlet 2| Iandwater Iout-let i223. Obviously, other cooling mediums beside water may be used in the jacket I9. The lower end of the jacket I3 is cylindrical in cross-section,

tapering gradually inwardly .from the -point 21 to the bottom thereof 29. rPhe outer `surfaceqof the portion 25 is ground in order to snugly '-ft in the upper end 3l of a condensate receiving section 33 and make a vapor-tight .seal therewith. One end of the tube l5 is fused to the wall of the upper end 3l.

The lower portion-of thecondenser Il is formed with an up-turned tube 35 of same cross-section as the tube l5 and is yaligned therewith to form a continuous passageway from the `axial passageway 3 to the condenser l1. The tube-35 has a small hole 3l at the bottom thereof in order-to permit any condensate which collects therein to escape and drop vinto the bottom -of the condenser I l.

The upper end of the condenser vll is formed with a tube 39 which in turn is yconnected -by means of neoprene tubing or other suitable vtubing to the pressure equalizing line 4|. The bottom of the pressure equalizing line 4I is in turn connected to the upper end of tube 43 by means of neoprene tubing or lother suitable connection. The lower end of ltube 43 has an enlarged portion 45 and a ground glass fitting 41 adapted to be inserted into a receiver (not shown) for collection of gas and condensate so that the fitting il makes a vapor-tight :joint with 'the receiver.

The bottom .of the acondenser 2| 1 is formed with -an open-ended downwardly lextending tubular portion 49 extending below the bottom 29 of the portion 25 of the jacket I9. A funnel 5I is supported immediately below the bottom of the tubular portion 49 by means of a non-corrosive and preferably non-magnetic, metallic pin 53 passing horizontally through holes adjacent the bottom of the tubular portion 49 and adjacent the upper lip of the funnel 5l. The outer ends of the pin 53 may be provided with glass beads 55 and 51 slipped thereon to keep the funnel centered in place. The funnel 5l is adapted to swing on the pin 53. The funnel 5l is formed with a side-ar-m 59 containing a core 6| of soft iron or other metal or alloy susceptible to magnetic impulses.

The bottom 63 of the condensate receiving section 33 is inclined and is formed integrally with an inclined tube 55 extending into the passageway 3 at a point below the bottom of thermometer well 1 in order to permit return of condensate through the passageway 3 and thence, to the distilling column. rhe tube 65 has a narrow portion 61 adapted to hold liquid therein by capillary attraction and prevent passage of vapor from the passageway 3 through the tube 65 into condensate section 33. The end of the tube 65 extending into the passageway 3 is provided with a drip tip 69 and a vent 'H on the upper surface thereof in order to provide for smooth delivery f condensate through passageway 3. The tube 65 is fused to the walls of both passageway 3 and jacket I.

The section 33 is also provided its bottoni and at a point diametrically opposite the point connected to the tube B5, with a bent tube lf3 having an open widened upper end l inside the Section 33 adjacent the wall thereof and a short distance below the bottom tip of the funnel 5I. The tube 'i3 is fused to the wall of the section 33. The tube 73 is bent to form a trap so that condensate collecting therein will form a seal. The outer end of the tube i3 is formed integrally with a ground glass ball joint il adapted to nt into a receiving jacket "lil which is in turn integrally connected to the end of an inclined tube 8l, the lower end of which extends into the enlarged portion t5. The end of the tube 8| extending into the enlarged portion d5 is formed with a drip tip St and a vent 85 on the upper side thereof in order to provide for smooth flow of liquid product into the collecting vessel. Another tube 8? connects the tube 3l at a point adjacent the joint 19 with the tube 43 immediately above the enlarged portion 45. A cooling jacket 89 is provided around tube il! through which a cooling medium may be circulated in order to prevent evaporation of any portion of the condensate withdrawn through the tube El.

As in the aforesaid Patent No. 2,251,185, an electromagnet (not shown) is provided outside condensate section 33 opposite the side-arm 59 of the funnel in order to swing the funnel as required at definite intervals of time. Any suit able timing device may be provided to regulate or vary reiiux ratio. For example, if a reflux ratio of 4 to 1 is desired, a device will vbe provided so that in 12 seconds the funnel will be permitted to hang vertically, in the position shown in the drawing, so that reflux from the condenser will pass through tube 65 back to the fractionating column, and then the funnel will be swung by energizing the magnet so that for the next three seconds the lower tip of the funnel is directly above the widened portion 'l5 of the tube 'I3 so that the condensate passes to the collector not shown.

As can be readily understood from the foregoing description and the accompanying drawing, temperature of the vapors leaving the distillation column is measured before they leave the vacuum jacketed vertical passageway 3 so that an accurate reading of the actual temperature can be obtained before any cooling effect occurs. Furthermore, it will be seen that the vapors enter directly into the condenser without any opportunity to undergo partial condensation prior thereto. Thus, the possibility of a portion of the vapor condensing as it leaves the distillation column and flowing back into the distillation column without passing through the funnel is avoided. By injecting the vapors directly into the condenser above the funnel, heating of the funnel is avoided with the consequent elimination of partial vaporization of the condensate in the funnel which inevitably results where a het atmosphere is maintained around the funnel. By suspending the funnel from the bottom of the condenser tube, a simplified construction is provided which permits easy operation of the funnel. By making the head in separate parts ease of packing for shipping purposes is provided and the apparatus can be readily repaired in the event the funnel gets out of order. The apparatus may be separated at points other than those described and illustrated by providing vapor tight joints at the points of separation. Moreover, breakage of one part does not necessitate replacement of the entire head. The elimination of the stopcock in the pressure equalizing line avoids the likelihood of inadvertently leaving the stopcock in closed position and disturbing the pressure balance in the distilling head.

By means of the improved dlstilling head shown and described, it is possible to obtain more enicient fractionating of laboratory samples and more accurate analysis thereof.

It is claimed:

1. A glass distilling head comprising, an insulated vapor passageway adapted to nt tightly on the top of a fractional distilling column, a condenser having a condensate outlet at the bottom thereof, a condensate receiving section below said condensate outlet and connected to said condenser means for passing vapor from said passageway directly to the bottom of said condenser above said outlet and bypassing said condensate receiving section, a pressure equalization line connecting the top of said condenser to said condensate receiving section a swingable funnel in said condensate receiving section positioned to permit the entire condensate from said condenser to pass therethrough, means for returning condensate from said funnel to the fractional distilling column, means to conduct condensate from said funnel to a collecting vessel, means to change the position of said funnel in order to permit said funnel to deliver condensate to either said vessel or to said fractional distilling column.

2. A distilling head in accordance with claim 1 in which the condensate receiving section is separate from the condenser and vapor passage and the condensate receiving section, vapor passageway and condenser are provided with vaportight joints adapted to fit together.

3. A glass distilling head for a fractional distilling column comprising an evacuated insulating jacket adapted to fit tightly in the top of said column and form a vapor tight seal therewith,

a vertical vapor passageway through said jacket connected to the top of the distilling column, a condenser having a condensate outlet at the bottom thereof the lower part of said condenser being connected above said outlet by a horizontal vapor passageway to the upper portion of said vertical passageway, a thermometer well in the top of said Vertical passageway extending below the point at which the horizontal passageway joins the vertical passageway, a condensate receiving section integral with said Vapor passageway but separate from said condenser and provided with means for removably mounting the bottom of said condenser in the top of said section by means of avapor-tight seal, a funnel swingably supported in said condensate receiving section from the bottom of said condenser directly below said outlet in such position as to cause the entire condensate from the condenser to pass through said funnel, means to convey condensate from said funnel to either said distilling column or to a collecting vessel and means for equalizing the pressure between said condenser and condensate receiving section.

4. A glass distilling head comprising, an insulated vapor passageway to t tightly on the top vapor exit of a fractional distilling column, a condenser having a condensate outlet at the bottom thereof, a condensate receiving section below said condensate outlet and connected to said condenser, means for passing vapor from said passageway directly to the bottom of said condenser above said outlet and bypassing said condensate receiving section, a swingable funnel in said -condensate receiving section positioned to permit the entire condensate from said condenser to pass therethrough, means for returning condensate from said funnel to the fractional distilling column, means to conduct condensate from said funnel to a collecting vessel, means to change the position of said funnel in order to permit said funnel to deliver condensate to either said vessel or to said fractional distilling column.

ALBERT W. GOLDSBARRY.

HOWARD S. MARTIN.

REFERENCES CITED The following references are of recordvin the le of this patent:

UNITED STATES PATENTS Number Name Date 2,251,185 Carter July 29, 1941 2,383,377 Evans Aug. 21, 1945 OTHER REFERENCES Industrial & Engineering Chemistry, Anal. ed., vol. 2, page 187, 1930. 

